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BLACK PRODUCTION FROM AND OF OF ASPHALTITE, TIRE AND

Yıldırım İ. Tosun

Mining Engineering Department, Şırnak University, Şırnak, Turkey [email protected]; [email protected] …

Abstract: , and oil is used as the raw material in the combustion production of black carbon by formations. Black carbon is useful with the increased surface area as soot or micro particles. It is traditionally believed that soot formation occurs in combustion of oil by certain amount of . As a result of this, a gas concentration gradient is needed between the carbon and the oxygen for soot production from the gaseous or liquid . Therefore, certain amount of carbon can only form for soot compounds that readily provide submicron black carbon product. Black carbon involves allotropic soot produced by not full combustion and removal of carbon matter in a closed-loop circulating batch system. This study searched that firstly, pyrolysis of low Şırnak asphaltite and washed with flotation device provided less ash Turkish lignites(less than 10% of the level in existing advanced clean lignite washery plant manufactured) with waste wood and tyre, secondly, combustion of pyrolysis oil of the for black carbon production on which the furnace gas parameters by examining the highest black carbon efficiency is obtained, and thirdly, according to the optimum design parameters of the pilot plant, gas furnace equipment investigated. The 32% soot yield from the 50% and 20%wood and 30% waste tyre weight rate were provided in the retort furnace. Keywords: coal pyrolysis, pyrolysis oil, coal soot, lignite pyrolysis, black carbon; pyrolysis oil

INTRODUCTION and type of fuel combustion, characteristics of furnace and combustion process configuration, and it can be optimized by varying the Lignite consumption of our natural resources in operational conditions (Rodriguez-Mirasol et al. energy production is increasing in parallel with 1994). the increasing energy needs today (IEA,2012). In terms of consumption and production Black carbon (BC) is widely used as fill for high quantities of our high-low thermal valuable quality tire production (Anonymous 2013, lignite reserves are limited (TKI 2009,TTK Anonymous 2009), also high conductive 2009). Depending on the economic technology graphite rods production, also as soot for enables the production of advanced production of paints and construction materials technological developments needed coal resistive . It may also thought as soot source derived products. Compliance with as activated carbon fill for treating wastewaters environmental norms coal pyrolysis or contaminated with phenols, volatile acids, facility allows the production of liquid aromatic and aliphatic organics. and gaseous needed with today's modern Basically better quality lignite oil production, high technology (Bell et al.2011). However, the value-added light oil, to produce black carbon method requires a variety of raw materials and products have been identified as key objectives. chemicals and adaptation to the type of For the production of black carbon, high amount processing fuel material. It has also been shown of oil (due to just about 7-20% production rate) that black carbon occurs during the time course is needed by the countries in the production of of diesel or other liquid fuel combustion pyrolysis lignite oil as much clean possible. processes that are based on bad combustion Acetylene is used to produce high quality soot (Shadle etal. 2001, Sharma etal. 2008). Most of black products in the reactor and (Amal et al. the studies aiming at black carbon quantifying 2010, Guerrero etal. 2005, Guerrero etal. 2008, performance were performed using offline Mendiara et al. 2007). Therefore further cleaning systems because of difficulties encountered in of Şırnak asphaltite and Turkish lignite, clean quantifying soot during combustion of ethylene product of pyrolysis with the production of liquid or waste rubber (Amal etal. 2011). Black carbon fuels will enable the development of South-East formation is dependent on several factors Anatolia and will also further enhance industrial including combustion parameters, temperature development and diversification and supply of Factors Affecting Pyrolysis and industrial energy fuel (Tosun 2012). Combustion for Black Carbon In this study, we are addressing the enhancement of soot formation by pyrolysis oil Effective processes depend on and CO2 gas, the definition and mechanisms of numerous factors including coal rank in combustion, the relationship between the carbonization, the volatile gaseous matter of temperature and CO2 gas partial pressure, the coal such as presence of , carbonyl factors affecting soot formation, the methods for gas and carbonization rate(Mendiara 2007) so determination and quantification of soot stabilizing the desorption, the settings of optimal formation and the mathematical models of diffusion conditions including structure defects combustion. Future research is still required to (, , , etc.), temperature, determine the optimum conditions for an oxygen content of coal, etc. and optimization of increased performance for other types of oil. concentration ratios (Amal 2011, Particularly, factors such as the black carbon Amal 2010) added the –desorption type, nature of the soot community and optimum balance, the residence time and the spatial process configuration need further investigation. distribution of molecules in coal pores among For this purpose it is necessary to provide basic other factors determining the efficiency of pilot knowledge of the industry working together carbonization. Guerrero et al. (2008) also with universities. Mainly due to improving yields included the carbon reactivity, the adsorption in performing quality raw materials and characteristics as factors affecting the rate and advanced processes for performance testing extent of carbonization much dependent on the processes according to the nature of our lignite- site activation, its gas desorption properties and to-date with research institutions and its porosity (Bell etal 2011). Carbonization is a technological applications are required. This prerequisite step for oil generation and soot study examined the beneficiation from our high- formation from tyre waste, biomass and sulfur lignite. However, technologies are coal. examined on the basis of lignite and lignite Coal particle size based on raw materials as well as the contribution of forest biomass and biogas plants A major reason is that the retention time in fixed waste cellulosic waste can be processed film processes is longer than in solid-gas together with our lignite in the contribution rate processes. This allows more time to the as 15-30%. carbonization for to the desorbed persistent compounds. Furthermore, high rank The modeling approaches and combustion with allows an sufficient intimate contact high CO gas content in combustion medium 2 between surface pores and gas atmosphere in other than the fuel type especially wood oil and the furnace due to more gas desorption (Kajitani pyrolysis oil of asphaltite. etal. 2006) Coal porosity PRODUCTION OF PYROLYSIS , The porous structure of activated carbon is a HEAVY OIL FROM COAL factor that determines to a great extent both the rate and degree of carbonization (Shadle et al., Many studies have investigated the numerous 2001). Sharma et al. (2008) found that, a advantages of adding pyrolysis oil to activated mesoporous coal was more efficiently combustion systems (Kegl 2011). The presence carbonized than a microporous coal. of carbon dioxide in conventional systems Phenol molecules that may undergo an improves soot settling, improves soot thickness, oxidative coupling reaction may be irreversibly increases soot removal, improves removal of adsorbed on coal, which in turn may result in soot, reduces the impact of organic shock low carbonization efficiency. Phenoxy radicals loadings, increases black carbon and oxygen formed by the removal of a hydrogen atom from concentration at the surface of soot carbon, each phenolic molecule can participate in direct increases removal, suppresses, improves, and coupling with other phenoxy radicals at even reduces bulking(Neeft et al. 1997). room temperature, coal surface serving as a In BC production, chemicals is enhanced catalyst. through the adsorption of inhibitory substances Carbonization efficiencies exceeding the total as in the catalytic processes, but in addition, the desorption abilities during increased fast BC used in the furnace serves as a supporting pyrolysis on coal and wood were also reported medium for iron film colon (Liu et al.2002, Wei- by Tosun (2013). Biao et al. 2001). Surface properties of coal - Reactivity On the other hand, in suspended growth systems, the use of BC is more advantageous (BET N ) specific surface area, total surface 2 than Granule BC since Powder BC systems activity, oxygen functional groups, total surface provide a uniform distribution of solids with a impurities, metal concentrations, dielectric value, minimum energy requirement for grinding. free radical concentration and reactivity of coal were related to the carbonization activity. In summary, in spite of the contradictory However, in some investigations, the pore size hypotheses, based on the available literature, it distribution of coal is also greatly to affect appears that pyrolysis of oil can occur when the pyrolysis kinetics (Guerrero etal. 2005). condensate is removed from the liquid phase through carbonation activity either in low or high temperature processes. Certainly, a oil Combustion of Pyrolysis Oil of Waste concentration gradient should establish for a Tire, Wood and Biomass continuing carbonation. Pyrolysis is extremely dependent on both carbonation and cracking Soot matter removal during BC treatments in coal. On the other hand, results from the combined effect of adsorption cracking reactions may increase the adsorbent and degradation. The efficiency of the combined of carbonyls. However, available data do not combustion–soot formation process is higher allow determining if the oil generation than expected for either soot formation or phenomenon depends solely on a mechanism production alone. Black carbon (BC) provides an involving absorption or if it also involves pore attachment surface for pollutants and protects activities. Further work is required to support them from shock loadings of toxic and inhibitory either one of these hypotheses. materials, whereas the black carbon. High processes using catalyst carbon as carrier for iron film attachment are efficient soot from Production of Black Carbon from ethylene. However, in catalytic systems the gas Pyrolysis Oil attachment to surface is less efficient than in iron film or in fluidized bed reactors using CO2 and pellets as iron film carrier (Jess etal. 2009, Oil Combustion Schurtz etal. 2009). This is because, in the latter, then retention time of solids is generally Considerable black carbon production on oil much higher than in black carbon processes, combustion and natural gas is managed as seen allowing more time for gas attachment to BC. in Figure 1.

Figure 1, Use of fuel gas and pyrolysis oil subjected to black carbon production flowsheet.

The research over coal pyrolysis and pyrolysis modeling assumes basically first-order gasification has been conducted over the years, kinetic equations, or less sensitive for heating but the pyrolysis results are widely dispersed rate (Donskoi et al. 1999). The other distributed because of the complex chemistry of coal (Bell activation model is dependent on the heating 2011, Kajitani etal. 2006). Time related coal- rate. The last two more advanced models need three and four constants, respectively, which Table 1,. Proximate Analysis of Turkish Lignite and basically depend on the coal properties but also Asphaltite. (ADB:Air dried base. DB:Dried base, cover to some extent, the effect of heat-and- DAB:Dried ashless base). mass transfer phenomena (Liu et al. 2011). The Coal Type Ash, Moisture, TotalS,% Volatile reaction rate of is influenced mainly by % % ADB DB Matter, chemical and physical factors, which include ADB % DAB coal type, catalytic effect of the ash and the Şırnak Asphaltite 6.3 0.1 5.7 52.6 specific surface area of char(Çakal et al. 2007), which changes during the reaction course with Kütahya Gediz 26.0 11.7 4.6 42.7 the development of internal pores, and finally, Soma Lignite 13.8 14.0 2.2 40.4 their destruction (Wiktorsson et al. 2000). In the Waste Wood 0.2 51.7 0.6 22.7 case of the scaling-up procedure, the Waste Tyre 13.8 0.01 0.2 60.4 uncertainty of a complex model of the reacting system may be very high and it is reasonable under some conditions to use a methodology based on quasi-equilibrium conditions, which can be reflected at a larger scale.

MATERIALS&METHOD

The representative samples were taken from local areas of the lignite. Fundamentally, the conditions regarding better desulfurization way, high quality lignite oil production, high value light oil, and gas products were determined Figure 3 Pyrolysis of Coal and Waste Tyre to black at the goal of high fuel producing yield. carbon This study examined the high sulfur and ash This work is based on the assumption that the types of Kütahya Gediz lignite, Soma lignite, final process temperature is a decisive factor for Şırnak asphaltite and lignite by TGA analyzer as the required volatile-matter content in the char illustrated in Figure 2. being in a quasi equilibrium state with respect to the gas temperature. Instead of fluid bed combustion, packed bed gasification of coarse size coals is governed by chemical reactions on particle gas reactions. Combustion rates of Şırnak asphaltite were lower in comparison with biomass and lignite as seen in Figure 4 so that mass diffusion rates of gaseous materials to Şırnak asphaltite particle fundamentally control reaction kinetics.

100

% 90

Figure. 2 Combustion of and Waste Tyre oil 80 and Biomass oil to black carbon 70 Proximate analysis of studied Turkish lignites 60 y = -10,1ln(x) + 119,48 and Şırnak asphaltite and waste wood and tyre 50 are found as given in Table 1. Studied coals and y = -11,9ln(x) + 116,83 40 biomass, tire wastes carried out on slow y = -13,28ln(x) + 110,03 pyrolysis and pyrolysis oil subjected to black 30 carbon production in retort, as shown in Figure 20 10 mm Şırnak Asphaltite 3. 5 mm Şırnak Asphaltite Combustion Weight Reduction Weight Combustion 10 2 mm Şırnak Asphaltite The country needs the cleanest fuel to be 0 produced providing the essential oils and gases. 1 10 100 1000 For this reason, gasification of Kütahya Gediz, Time, s Soma lignite, Şırnak asphaltite and lignite may Figure 4, Combustion kinetics of Şırnak Asphaltite for be so feasible at the side of cost and production black carbon production high amount of gaseous fuels instead of importing natural gas. A kiln reactor was used in coal pyrolysis heated Quantification based on measurement collected till 600oC with a rate 7-10oC/min by fuel. The the weights of black carbon and char products process was tested at a scale of 2–3 kg/h; are determined at each combustion and collecting operational and design data to build pyrolysis tests. an industrial installation. A technological Flue gas soot conversion by CO medium and diagram of the coal pyrolysis process developed 2 temperature control in fluidized chamber are unit is made. carried out. Produced pyrolysis oils were Thermal destruction almost observed at combusted in the reactor as illustrated in Figure temperature increase from 350 °C to 400°C with 5. in a batch black . This approach is pyrolysis rate of 60-70% and with simultaneous accurate, fast, and allows determination of time- dilution of oil products by condenser distillate. course experimental parameters. In this case, To achieve this, it is necessary to create loaded BC is centrifuged and transferred to conditions of internal circulation without the batch cell. Controls of unloaded BC with and transported coal and char in rotary kiln, where loaded BC without are run in parallel. When the the average concentration of solids amounts to CO2 curves reach a stable level indicating that 0.1- 0.2 kg/m3. reactivity had ceased, the less carbon dioxide consumed. it is necessary to create gaseous conditions for black soot formation in retort without the transported coal and char back in retort, where the average concentration of solids amounts to 0.1- 0.2 kg/m3 and the conditions for residence time are long enough for the combustion of coal and intensive gas mixing so enhancing mass and heat transfers. Thermal pyrolysis commenced by oil and tar fuel burning into the retort firstly and then CO2 gas evolution followed and circulated into the retort for three hours. When it is observed a temperature increase from 600 to 700°C without Figure 5, Combustion of pyrolysis oil of Coal, Waste fuel addition, injected cooling water at a volume Tyre oil, Biomass oil and flue gas to black carbon rate of 2/1 and air with 3lt/min. Gaseous Pyrolysis oil and tar of Kütahya Gediz lignite products with simultaneous dilution of oil Şırnak asphaltite and waste tyre were products by condenser distillate are collected. combusted in flash chamber each separately To achieve this, it is necessary to create and conversion to char determined as weight conditions of internal circulation without the collected in the cylone downstream. The results transported coal and char in retort; about 10- are illustrated in Figure 6. 20% very low conversion yields to black carbon were observed at the end of pyrolysis. 30 Şırnak Asphaltite Waste Tyre Kütahya Gediz Lignite 25

The Kinetics of Combustion to Soot y = 4,7358ln(x) - 0,154

Reactivity can be determined from CO2 20 conversion of solid carbon source in black carbon production medium for batch black carbon combustion. This approach is accurate, 15 fast, and allows determination of time-course experimental parameters. In this case, loaded 10 y = 3,3173ln(x) + 0,4411 BC is centrifuged and transferred to batch cell. % Conversion Soot Controls of unloaded BC with and loaded BC 5 y = 0,1031x + 3,3575 without are run in parallel. When the CO2 curves reach a stable level indicating that reactivity had ceased, the carbon consumed. 0 1 10 100 1000 Oxygen Uptake also shows the kinetics of Time, s indirectly soot conversion and directly reaction Figure 6, Pyrolysis soot conversion of Gediz lignite at rate of combustion and control, even cooling equal weight rate separately in Pyrolysis Retort in water addition and fuel gas inlet. comparison with Waste tyre

Oxygen consumption was the indication of soot RESULTS AND DISCUSSION conversion of oil combustion and change of oxygen uptake in the tests was shown in Figure 7. The results of conversion of soot and char with combustion of flue In the pyrolysis experiments with addition waste tyre, the reactor temperature was changed gas of pyrolysis and pyrolysis oil of coal, waste tire o o and waste wood as shown in Figure 8. between 400 C and 700 C and lignite samples were mixed with only by weight rate of 10% 14 Şırnak Asphaltite Tar Waste Tyre Tar waste tire and waste wood. Products received from pyrolysis and combustion of coal and 12 Gediz Lignite Tar 10 waste mixtures were subjected to analysis for soot and char weight determination. Test results y = -25,394x + 11,487 8 of pyrolysis by waste tire and separately waste o 6 y = -12,687x + 6,5733 wood at 600 C are seen in Figure 3.

4 From the point of view of pyrolysis and oil Oxygen Uptake,% Oxygen 2 combustion experimentation, the resulted soot y = -13,866x + 5,5316 0 and quality and quantity in the pyrolysis 0 0,1 0,2 0,3 0,4 chambers for biomass, lignite and coal-waste Time,min mixture samples were determined for different Figure 7, Combustion kinetics of Coal gas and Waste source evaluation and so we may reduce the Tyre oil and Biomass oil to black carbon effect of ash and sulfur content of coal samples in order to optimize pyrolysis and combustion 50 rates of lignite samples. As given in Figure 5 gas 45 and oil yields for lignite and coal samples were 40 slightly similar, oil yield was lower for coal. In the

35 pyrolysis experiments with different particle size 30 fractions of coal specimens, at reactor temperature changed to 600oC and lignite 25 samples mixed only by waste tyre at 10% weight 20 Şırnak Asphaltite+ %25 Waste Tire rate. Products of pyrolysis of coal specimens 15 Şırnak Asphaltite+25% Waste Wood were subjected to analysis for yield 10 Soot Yield Ratio ,%Ratio Yield Soot Şırnak Asphalite determination. 5 Soma Lignite Test results of pyrolysis of Turkish lignite are 0 Gediz Lignite seen in Figure 4. Comparison of particle size at 400 500 600 700 Pyrolysis Temperature,oC 3-10mm additions at equal rates into the pyrolysis chamber with finer lignite showed that Figure 8, Combustion kinetics of Coal gas and Waste Gediz lignite was showed higher oil yield at near Tyre oil and Biomass oil to black carbon 26 % weight rate. In the gasification Quality of Black Carbon produced from experiments, the experimental condition is Pyrolysis Oil calculated on the basis of the gas composition in the ambient state. So neither the contained BET N2 surface area analysis and pour density water vapour nor the condensing hydrocarbons size analysis were determined and compared are taken into account. However, these trade class black carbons in order to ascertain components increased by decrease the particle usage type. Based on measurement of black size to 100 micron and oil yield was remained carbon quality over test products, ash content low 12% weight. Those values provided and sulfur contents were also determined and advantageous higher carbonaceous content to the results are given in Table 2. be converted to gas in gasification stage. Table 2, Black Carbon Qualities produced from Pyrolysis liquid and gaseous products of Sırnak Combustion of Pyrolysis Oil of Coal. asphaltite may equal to 5–20 g tar/m3 and 5–10 g /m3 of , toluene, xylene in unit Coal Type Trade Aphaltite Soma Tar Gediz process gas. Moreover, Figure 5 showed that oil BC Tar BC BC Tar BC yields was slightly lower than coal char yields N2 Surface area 53 27 23 21 27% weight. Gas yield was containing mainly m2/g steam and CO2 in the pyrolizer and the amount Ash content % 0,20 0.3 0.6 0.7 of gas was remained between 37 and 40%. Sieve residue 0,01 0,01 0,04 0,04 Combustion tests were carried out for pyrolysis (100mesh) oil and tar of Turkish lignite and Şırnak Pour Density 340 320 380 340 asphaltite and optimized gas inlet of 3lt/min.kg coal tar. Soot yields for Turkish lignite and Şırnak asphaltite across to temperature were shown from Figure 8 and even other lignites Acknowledgements showed similar trend, the higher char yields at lower combustion temperatures. it is illustrated The author would like kindly thanks to Alfa that higher carbonaceous content to be Kazan Makina A.Ş., ANKARA for providing great converted to gas in gasification was managed concerns and supports. over 650oC till 700oC. That conversion rate remained among 28-36%. Even it was observed that increased the gas's calorific value by up to References approximately 3200 kJ/m3 at 700oC for Şırnak asphaltite. 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